CN108822815A - A kind of preposition gel of well cementation - Google Patents
A kind of preposition gel of well cementation Download PDFInfo
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- CN108822815A CN108822815A CN201810432046.9A CN201810432046A CN108822815A CN 108822815 A CN108822815 A CN 108822815A CN 201810432046 A CN201810432046 A CN 201810432046A CN 108822815 A CN108822815 A CN 108822815A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/44—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing organic binders only
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Abstract
The present invention provides a kind of preposition gel of well cementation, the component including following mass parts：100 parts of epoxy resin solution, 10~20 parts of resin curing agent, 5~10 parts of retarder, 0.2~0.5 part of swelling agent, 5~10 parts and 100~110 parts of heavy weight additive of emulsifier.Embodiment the result shows that, provided by the invention cement the well will not influence the consistency of cement slurry with preposition gel, with excellent elasticity, the closing to fluid-channeling channel is further realized in grout cures layer upper end, the annular channeling and annular space problem with pressure effectively during prevention well cementing operation.
Description
Technical field
The present invention relates to Cementing technical field more particularly to a kind of preposition gels of well cementation.
Background technique
Annular space with pressure is the phenomenon that well cementing operation process usually occurs.The annular space annular pressure with pressure referred at well head passes through
The phenomenon that stress level before pressure release is restored to after pressure release again.What oil/gas well was all made of plurality of layers casing, it constitutes several
A annular space.Gas well annular space is with pressure mainly following reason：First is that due to various artificial origins (including gaslift, thermal recovery management,
Monitor annular pressure or other purposes) caused by annular space it is with pressure；Second is that casing annulus temperature change and ballooning effect cause to flow
Body and expansion pipe column deformation cause annular space with pressure；Third is that since there are gas channelling to cause annular space with pressure for annular space.Finally, tubing and casing
The annular space that column failure is especially threadedly coupled and packer sealing failure causes gas channelling to be formed is with pressure.The annular space that operation applies
Pressure and by temperature change make annular fluid expand caused by annular pressure can be eliminated after well head pressure release, tubing and casing string failure
It can also be eliminated by replacement tubing string after being diagnosed, but annular pressure caused by has channeling may continue to exist after well head pressure release,
With permanent.
Annular channeling is equally the potential engineering technology that all gas well cementing processes will face after well cementing operation
Problem, serious annular channeling or annular space it is with pressure not only make subsequent well operation, perforating job, workover treatment, test jobs with
And well stimulation cannot smoothly be implemented, and can also constitute a threat to the safe working of well construction period, oil gas.If annular space channelling can not be controlled
System, it will lead to blowout, in some instances it may even be possible to cause full well to be scrapped, cause huge economic loss.In addition, if annular space value with pressure is super
The intensity that sleeve design can bear is gone out, has also resulted in casing collapse, equally will cause significant damage.
The prior art mainly adopts active curing cement technologies to solve the problems, such as that annular channeling and annular space are with pressure, for example,
Schlumberger (Schlumberger) company will have investigated what the active curing cement of FUTUR and Halliburton Company released
LifeCem or LifeSeal cement.Annular space is there are when oil gas channelling, in the case where no ground artificial is intervened, cement sheath energy
It is expanded, fluid-channeling channel can be closed；This self-sealing characteristics of cement sheath are by the way that extraordinary additive is added in cement slurry
Come what is realized.Brittleness is larger after active curing cement solidification in the prior art, easily loses well cementation effect, hinders and makees to well cementation
The solution of annular channeling and annular space problem with pressure during industry.
Summary of the invention
In view of this, the present invention provides a kind of preposition gels of well cementation.The preposition gel of well cementation provided by the invention has
Excellent elasticity further realizes the closing to fluid-channeling channel in grout cures layer upper end, effectively prevents well cementing operation process
In annular channeling and annular space problem with pressure.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preposition gel of well cementation, the component comprising following mass parts：
The preparation method of epoxy resin includes the following steps in the epoxy resin solution：
(1) epoxy propane butyl ether, butyl acrylate, phloroglucin and deionized water are mixed, carries out polycondensation reaction, obtains
To epoxy resin precursor；The temperature of the polycondensation reaction is 80~90 DEG C, and the time of polycondensation reaction is 3.5~4.5h；
(2) the epoxy resin precursor that the step (1) obtains is mixed with alkaline solution, carries out ring-closure reaction, obtains
Reaction material liquid；The temperature of the reaction is 83~87 DEG C, and the time of reaction is 2.5~3h；
(3) reaction material liquid that the step (2) obtains successively is washed and is dried, obtain epoxy.
Preferably, the mass ratio of step (1) the oxypropylene butyl ether, butyl acrylate, phloroglucin and water is
(14.9~15.1)：(14.9~15.1)：(29.9~30.1)：(19.9~20.1).
Preferably, the mass concentration of the alkaline solution is 30%；With the epoxy resin precursor preparation epoxy third
The mass ratio of the meter of alkane butyl ether, the alkaline solution and epoxy propane butyl ether is (5.9~6.1)：(14.9~15.1).
Preferably, the resin curing agent is organic amine curing agent.
Preferably, the organic amine curing agent includes one of aliphatic amine, polyamide and aromatic amine or a variety of.
Preferably, the retarder includes in sodium glucoheptonate, boric acid, xylonic acid and acid-co-maleic acid
It is one or more.
Preferably, the swelling agent includes sodium hydroxide, silicon alunite, calcium sulphoaluminate, calcium oxide, fe, calcium oxide-
One of calcium sulphoaluminate compound is a variety of.
Preferably, the emulsifier is fatty alcohol polyethenoxy ether class compound.
Preferably, the heavy weight additive includes barite or Iron Ore Powder.
The present invention provides a kind of preposition gel of well cementation, the component including following mass parts：Epoxy resin solution 100
Part, 10~20 parts of resin curing agent, 5~10 parts of retarder, 0.2~0.5 part of swelling agent, 5~10 parts of emulsifier and heavy weight additive 100
~110 parts.After well cementation provided by the invention is mixed with preposition gel with cement slurry with arbitrary proportion, to mutual rheology, thickening
The basic performances such as time do not impact substantially, i.e., influence that less, cement slurry sealing upper end hair can be stable in the presence of between each other
It waves the closing to fluid-channeling channel, and then effectively prevents the annular channeling during well cementing operation and annular space is with pressure.
Specific embodiment
The present invention provides the present invention provides a kind of preposition gel of well cementation, the component comprising following mass parts：
The preparation method of epoxy resin includes the following steps in the epoxy resin solution：
(1) epoxy propane butyl ether, butyl acrylate, phloroglucin and deionized water are mixed, carries out polycondensation reaction, obtains
To epoxy resin precursor；The temperature of the polycondensation reaction is 80~90 DEG C, and the time of polycondensation reaction is 3.5~4.5h；
(2) the epoxy resin precursor that the step (1) obtains is mixed with alkaline solution, carries out ring-closure reaction, obtains
Reaction material liquid；The temperature of the reaction is 83~87 DEG C, and the time of reaction is 2.5~3h；
(3) reaction material liquid that the step (2) obtains successively is washed and is dried, obtain solid epoxy.
In the present invention, such as without particular/special requirement, well cementation raw material used in preposition gel is those skilled in the art
Commercial goods known to member.
The preposition gel of well cementation provided by the invention includes 100 parts of epoxy resin solution in terms of mass parts.In this hair
In bright, the epoxy resin solution is the mixture of solid epoxy and organic solvent；Epoxy in the epoxy resin solution
The mass ratio of resin and organic solvent is preferably 1:1；The organic solvent is preferably ethyl alcohol, ethers or acetone.The present invention is preferred
By mixing the epoxy resin and organic solvent, epoxy resin solution is obtained.
In the present invention, the preparation method of epoxy resin includes the following steps in the epoxy resin solution：
(1) epoxy propane butyl ether, butyl acrylate, phloroglucin and water are mixed, carries out polycondensation reaction, obtains epoxy
Resin precursor；The temperature of the polycondensation reaction is 80~90 DEG C, and the time of polycondensation reaction is 3.5~4.5h；
(2) the epoxy resin precursor that the step (1) obtains is mixed with alkaline solution, carries out ring-closure reaction, obtains
Reaction material liquid；The temperature of the reaction is 83~87 DEG C, and the time of reaction is 2.5~3h；
(3) reaction material liquid that the step (2) obtains successively is washed and is dried, obtain epoxy resin.
In the present invention, the mass ratio of the epoxy propane butyl ether, butyl acrylate, phloroglucin and water is preferably
(14.9~15.1)：(14.9~15.1)：(29.9~30.1)：(19.9~20.1), further preferably 15:15:30:20.
The present invention mixes epoxy propane butyl ether, butyl acrylate, phloroglucin and water, carries out polycondensation reaction, obtains epoxy resin
Precursor, i.e. polyphenol base ethylene oxidic ester (alcohol ether intermediate).In the present invention, the temperature of the polycondensation reaction be preferably 80~
90℃；The time of the polycondensation reaction is preferably 3.5~4.5h, further preferably 4h.In the present invention, the water is preferably
Deionized water；The introducing of impurity is avoided using deionized water.
After the polycondensation reaction, the polycondensation reaction feed liquid is preferably carried out natural cooling by the present invention, obtains epoxy resin
Precursor；The final temperature naturally cooled to is preferably room temperature, and further preferably 10~20 DEG C.The present invention is in cooling
Afterwards, it after then being mixed with lye, then is warming up to reaction temperature needed for next step and is reacted, can be avoided direct hybrid reaction too
Acutely.
After obtaining epoxy resin precursor, the present invention mixes the epoxy resin precursor with alkaline solution, is closed
Ring reaction, obtains reaction material liquid.In the present invention, the alkaline solution and epoxy resin precursor preparation propylene oxide butyl
The mass ratio of ether is preferably (5.9~6.1)：(14.9~15.1), further preferably 6：15, the quality of the alkaline solution is dense
Degree preferably 30%.In the present invention, the alkaline solution is preferably sodium hydroxide solution or potassium hydroxide solution.In the present invention
In, the epoxy resin precursor and alkaline solution preferably react 3h under the conditions of 85 DEG C, contain ring in obtained reaction material liquid
Oxygroup phenolic group ethylene oxidic ester and epoxy resin；The reaction temperature of the epoxy resin presoma and alkaline solution is further preferred
It is 83~87 DEG C；Reaction time is more preferably 2.5~3h.
After obtaining reaction material liquid, obtained reaction material liquid is successively washed and is dried by the present invention, obtains solids epoxy
Resin.In the present invention, the number of the washing is more than three times；The washing can wash off remaining lye.The present invention
There is no particular/special requirement to the specific embodiment of the drying, so that the moisture content of dried product exhibited is 1% hereinafter, not having
Solids adhering is in glassware；In the present invention, the temperature of the drying is preferably 80~90 DEG C；The dry time is preferred
For 2~3h.
In the present invention, epoxy resin elasticity with higher is avoided directly being solidified using conventional epoxy and be led
Cause greater hardness and brittleness.In the present invention, the epoxy resin has certain malleable, when by has channeling gas pressure
When, pit shaft can be effectively insulated, is avoided because of cracking caused by embrittlement.
On the basis of 100 mass parts of the epoxy resin solution, the preposition gel of well cementation provided by the invention includes 10
~20 parts of resin curing agent, preferably 12~18 parts, further preferably 15~16 parts.In the present invention, the resin is solid
Agent is preferably organic amine curing agent；Organic amine curing agent preferably includes one in aliphatic amine, polyamide and aromatic amine
Kind is a variety of；The aliphatic amine further preferably includes diethylenetriamine and/or ethylenediamine.In the present invention, described organic
Amine curing agent realizes the adjustment to resin curing time and solidification intensity, can satisfy to the regulation of the curing time of resin existing
Field pumping requirements, so that possessing good mobility before reaching stratum, good intensity can effectively resist strata pressure
Impact.
On the basis of 100 mass parts of the epoxy resin solution, well cementation provided by the invention with preposition gel comprising 5~
10 parts of retarder, preferably 6~8 parts.In the present invention, the retarder preferably includes sodium glucoheptonate, boric acid, xylonic acid
With one of acid-co-maleic acid or a variety of.When retarder includes boric acid, xylonic acid and organic phosphate and Malaysia
When the copolymer of acid, the present invention does not have particular/special requirement to the relative usage of each component in the mixture.In the present invention, described slow
Solidifying agent further realizes the adjustment to resin curing time, effectively delays the preposition gel under the action of resin curing agent
Curing time so that being pumped to resolidification behind stratum.
On the basis of 100 mass parts of the epoxy resin solution, the preposition gel of well cementation provided by the invention includes 0.2
~0.5 part of swelling agent, preferably 0.35~0.4 part.In the present invention, it is bright to preferably include sodium hydroxide, silicon for the swelling agent
One of aluminite, calcium sulphoaluminate, calcium oxide, fe, calcium oxide-calcium sulphoaluminate compound is a variety of.In the present invention, institute
Stating the mass ratio of calcium oxide and calcium sulphoaluminate in calcium oxide-calcium sulphoaluminate compound is preferably (1~2)：(1~2).In the present invention
In, the swelling agent avoids resin after solidification from generating contraction, and then effective seal shaft as expanding material.
On the basis of 100 mass parts of the epoxy resin solution, well cementation provided by the invention with preposition gel including 5~
10 parts of emulsifier, further preferably 6~8 parts.In the present invention, the emulsifier is preferably fatty alcohol polyethenoxy ether class
Compound, further preferably fatty alcohol polyoxyethylene ether OE-2, fatty alcohol polyoxyethylene ether OE-4, fatty alcohol polyoxyethylene ether
One of OE-6 and fatty alcohol polyoxyethylene ether OE-70 or a variety of.In the present invention, the emulsifier helps to improve resin
Stability, when well cementation in preposition gel use process on cement slurry confining bed top, can be with grout cures confining bed
It is steadily contacted, improves the well cementation stability of the gel rubber system and cement paste mixture.
On the basis of 100 mass parts of the epoxy resin solution, the preposition gel of well cementation provided by the invention includes 100
~110 parts of heavy weight additive, further preferably 105~108 parts.In the present invention, the heavy weight additive preferably include barite or
Iron Ore Powder.In the present invention, the partial size of the barite is preferably 150~200 mesh, further preferably 170~185 mesh；Institute
The partial size for stating Iron Ore Powder is preferably 250~1200 mesh, further, the Iron Ore Powder be Iron Ore Powder that partial size is 250 mesh and
The Iron Ore Powder of 1200 mesh is according to 3:1 mass ratio configures.In the present invention, the addition of the heavy weight additive, can be improved resin
Density, be pumped into stratum convenient for the preposition gel, balance stratum pore pressure, realization consolidates stratum.In the present invention,
The well cementation is preferably 1.9g/cm with the density of preposition gel3。
The present invention cements the well described in above-mentioned technical proposal does not have any particular/special requirement, energy with the preparation method of preposition gel
It is enough to be uniformly mixed each raw material.The raw material is preferably obtained preposition gel of cementing the well by the present invention after evenly mixing；Into
One step is preferably：Heavy weight additive is added after resin, resin curing agent, retarder, swelling agent and emulsifier are mixed.
The present invention does not have particular/special requirement to the specifically used mode for cementing the well preposition gel, using those skilled in the art
Cementing concrete application mode known to member.In the present invention, the application mode of the preposition gel of cementing the well is further
Preferably：Well cementation is treated using cement slurry to be closed, and cement sheath is obtained；The preposition gel is added on the cement sheath
End is contacted with cement sheath.The present invention in the wellbore cement sheath upper section increase by one section of gel rubber system, consolidate strata pressure, pre- gas-tight
It alters.
In the present invention, the cement slurry is preferably cementing slurry；The present invention is to the composition of the cement slurry without spy
It is different to require, the cement slurry well-known to those skilled in the art for well cementation.In the present invention, the cement slurry preferably wraps
Include the component of following mass parts：100 parts of G class g cement, 46.25 parts of fresh water, 2.25 parts of fluid loss additive, 0.5 part of dispersing agent, reinforcing agent
1.5 parts, 1.25 parts of swelling agent, 2 parts of toughener, 0.63 part and 0.5 part of defoaming agent of retarder.
In the present invention, the model of the G class g cement is preferably JH or SX；Fluid loss additive is preferably in the cement slurry
FLO-S；The dispersing agent is preferably DISP-S；The reinforcing agent is preferably STR；The swelling agent is preferably bond；The increasing
Tough dose of preferably Latex；The retarder is preferably H21L；The defoaming agent is preferably DESIL.In the present invention, the water
The density of mud is preferably 1.90g/cm3。
The preposition gel of well cementation provided by the present invention and cement slurry have good compatibility, can be with any with cement slurry
Ratio mixing, and cement slurry will not be polluted, it is seen that working security with higher.In the present invention, before the well cementation is used
Set in gel and the test of cement slurry compatibility, the mass ratio of the two be preferably (0,10]：[10,0), further preferably (1~
9)：(9~1).
Well cementation provided by the invention is described in detail with preposition gel below with reference to embodiment, but cannot be it
Be interpreted as limiting the scope of the present invention.
Previously prepared epoxy resin：By the epoxy propane butyl ether of 10 parts by weight, the butyl acrylate of 15 parts by weight, 30 weights
Measure the phloroglucin of part, the deionized water of 20 parts by weight is proportionally added into reaction kettle, 80 DEG C of reaction 4h, cold after fully reacting
But to 40 DEG C, 6 parts by weight 30wt% sodium hydroxide solutions are then added thereto, 3h are further reacted at 85 DEG C, after cooling
Resulting material is washed, then the dry 2h at 80~90 DEG C, obtains solid resin beads, add according to hard resin
With ethyl alcohol quality 1:1 ratio is dissolved in ethyl alcohol to get epoxy resin solution.
Used epoxy resin is all made of this epoxy resin solution in following example 1~8.
Embodiment 1：
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 17 parts by weight of resin curing agent, 9 weight of retarder
Part, 0.6 parts by weight swelling agent, 5 parts by weight of emulsifier, 106 parts by weight of heavy weight additive.Wherein, resin is the Breakup of Liquid Ring being prepared
Oxygen resin, resin curing agent are aliphatic amine, retarder is sodium glucoheptonate, swelling agent is 0.1 mass parts simple substance silica flour and
Mixture, emulsifier OE-70, the heavy weight additive of the 20wt.% sodium hydroxide solution of 0.5 mass parts are Iron Ore Powder.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 2
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 20 parts by weight of resin curing agent, 9 weight of retarder
Part, 0.6 parts by weight swelling agent, 5 parts by weight of emulsifier, 106 parts by weight of heavy weight additive.Wherein, resin is the Breakup of Liquid Ring being prepared
Oxygen resin, resin curing agent are aliphatic amine, retarder is sodium glucoheptonate, swelling agent is 0.1 mass parts simple substance silica flour and
Mixture, emulsifier OE-70, the heavy weight additive of the 20wt.% sodium hydroxide solution of 0.5 mass parts are Iron Ore Powder.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 3
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 17 parts by weight of resin curing agent, 5 weight of retarder
Part, 0.6 parts by weight swelling agent, 5 parts by weight of emulsifier, 106 parts by weight of heavy weight additive.Wherein, resin is the Breakup of Liquid Ring being prepared
Oxygen resin, resin curing agent are aliphatic amine, retarder is sodium glucoheptonate, swelling agent is 0.1 mass parts simple substance silica flour and
Mixture, emulsifier OE-70, the heavy weight additive of the 20wt.% sodium hydroxide solution of 0.5 mass parts are Iron Ore Powder.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 4
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 17 parts by weight of resin curing agent, 10 weight of retarder
Part, 0.6 parts by weight swelling agent, 5 parts by weight of emulsifier, 106 parts by weight of heavy weight additive.Wherein, resin is the Breakup of Liquid Ring being prepared
Oxygen resin, resin curing agent are aliphatic amine, retarder is sodium glucoheptonate, swelling agent is 0.1 mass parts simple substance silica flour and
Mixture, emulsifier OE-70, the heavy weight additive of the 20wt.% sodium hydroxide solution of 0.5 mass parts are Iron Ore Powder.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 5
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 17 parts by weight of resin curing agent, 9 weight of retarder
Part, 0.6 parts by weight swelling agent, 5 parts by weight of emulsifier, 106 parts by weight of heavy weight additive.Wherein, resin is the Breakup of Liquid Ring being prepared
Oxygen resin, resin curing agent are aliphatic amine, retarder is sodium glucoheptonate, swelling agent is 0.1 mass parts simple substance silica flour and
Mixture, emulsifier OE-70, the heavy weight additive of the 20wt.% sodium hydroxide solution of 0.5 mass parts are Iron Ore Powder.
Raw material mixes under the conditions of 90 DEG C, obtains preposition gel of cementing the well.
Embodiment 6
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 10 parts by weight of resin curing agent, 5 weight of retarder
Part, 0.2 parts by weight swelling agent, 5 parts by weight of emulsifier, 100 parts by weight of heavy weight additive.Wherein, resin is organic siliconresin, and resin is solid
Agent is polyamide, and retarder is boric acid, swelling agent is calcium oxide, emulsifier is aliphatic acid polyethenoxy ether OE-2, heavy weight additive
For barite.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 7
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 20 parts by weight of resin curing agent, 10 weight of retarder
Part, 0.5 parts by weight swelling agent, 10 parts by weight of emulsifier, 110 parts by weight of heavy weight additive.Wherein, resin is phenolic resin, and resin is solid
Agent is aromatic amine, and the iron filings that retarder is xylonic acid, swelling agent is 1200 mesh of 250 mesh of partial size and partial size are according to 3:1 mass ratio
Mixing iron filings, emulsifier are aliphatic acid polyethenoxy ether OE-4 made of configuration, heavy weight additive is barite.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Embodiment 8
It cements the well the preparation of preposition gel：100 parts by weight of epoxy resin, 10 parts by weight of resin curing agent, 10 weight of retarder
Part, 0.5 parts by weight swelling agent, 10 parts by weight of emulsifier, 110 parts by weight of heavy weight additive.Wherein, resin is organic siliconresin, resin
Curing agent is aromatic amine, and retarder is boric acid, swelling agent is aluminium calcium sulfate, emulsifier is aliphatic acid polyethenoxy ether OE-6, adds
Heavy prescription is barite.
Raw material mixes under the conditions of 80 DEG C, obtains preposition gel of cementing the well.
Comparative example 1
Preposition gel is prepared in the way of embodiment 1, difference is, uses conventional epoxies.
Shore hardness 90D is up to after the preposition gel solidification that comparative example 1 is obtained, without elasticity.
For hardness between 40-60D, elasticity is good after the preposition gel solidification that Examples 1 to 8 is obtained.
To Examples 1 to 8 be prepared well cementation with preposition gel carry out intensity, pump-conveying property and with the compatibility of cement slurry
Performance is detected；Wherein, the evaluation method of gel strength is：It is measured under different temperatures using MD-NJ5 gel strength measuring instrument
The intensity of the preposition gel of well cementation of crosslinked good (solidification)；The evaluation method of pump-conveying property is：Measurement is prepared at normal temperature
The rheological property of the good preposition gel of well cementation is the fast rotational viscometer of the sensible ZNN-D6A six in Qingdao sea using instrument.
With the evaluation method of the compatibility of cement slurry：The preposition gel rubber system of prepared well cementation and cement slurry are pressed into quality
Than 0:10,1:9,2:8,3:7,4:6,5:5,6:4,7:3,8:2,9:1,10:0 is mixed, and the difference of cement slurry is then measured
Thickening time and intensity under the conditions of temperature, the formula of the cement slurry for test are：The G class g cement of 100 mass parts, 46.25 matter
Measure the fresh water of part, the fluid loss additive FLO-S of 2.25 mass parts, 0.5 mass parts dispersing agent DISP-S, 1.5 mass parts enhancing
Agent STR, the swelling agent bond of 1.25 mass parts, the toughener Latex of 2 mass parts, 0.63 mass parts retarder H21L and 0.5
The defoaming agent DESIL of mass parts；The density of cement slurry is 1.90g/cm3。
The strength test results of the preposition gel of well cementation are as shown in table 1.
Intensity and thickening time of the well cementation that 1 Examples 1 to 8 of table obtains with preposition gel
As shown in Table 1, cementing fluid is pumped into time on stratum generally in two hours to three hours, during this period fluid
There should be good mobility, therefore the gel rubber system thickening time substantially conforms to site requirement；Gel strength is in 40N or so
When, stratum can be effectively insulated, prevents has channeling.
The pump-conveying property test result of the preposition gel of well cementation is as described in Table 2.
The pump-conveying property for the preposition gel of well cementation that 2 Examples 1 to 8 of table is prepared
Apparent viscosity is the Primary Reference data of the rheological property of the preposition gel, as shown in Table 2, before provided by the invention
The fluid for setting gel is diluter, good fluidity；Plastic viscosity reflects in laminar flow conditions, the destruction of epoxy resin weight grid structure
It is interior between the solid phase particles of suspension, between solid phase particles and liquid phase and inside Continuous Liquid Phase when with restoring in dynamic balancing
The power of rubbing action.
It is tested using well cementation wall surface and alters instrument, the packing performance of gel rubber system is evaluated, specific evaluation result is shown in Table 3.
It is known that by the analysis of table 3：After gel rubber system solidification, bearing capacity can reach 13MPa.Therefore, this kind of gel rubber system
Possess good packing performance, can achieve the purpose of anti-gas channeling.
3 gel rubber system of table insulates performance evaluation
Note：Well cementation consolidated model curing condition：60 DEG C × normal pressure × 96h.
The present invention provides preposition gel and cement slurry compatibility test result is as shown in table 4.
The preposition gel of 4 Examples 1 to 8 of table and cement slurry are in varing proportions after compatibility, thickening time statistical form
As shown in Table 4, the preposition gel of well cementation provided by the invention and cement slurry be in varing proportions after compatibility, gel it is strong
The thickening time of degree and cement slurry is able to maintain stabilization, it is seen that the preposition gel of well cementation and cement slurry compatibility are good, Bu Huiying
The well cementation effect of Xiangshui County's mud.
The well cementation that Examples 1 to 8 obtains is tested with the stability of preposition gel：The well cementation obtained is coagulated with preposition
Glue is placed in transparent glass cup, stands 3 days under room temperature, preposition gel does not have obvious sedimentation phenomenon, and rheological property is not by shadow
It rings, any special variation does not occur；It can be seen that well cementation having good stability with preposition gel provided by the invention.
Unrestricted compression verification evaluation Examples 1 to 8 is carried out using the omnipotent mechanics machine of material indoors to be prepared
Well cementation preposition gel solidification module elasticity, by the configured preposition gel of Examples 1 to 8 be respectively put into 80 DEG C ×
In curing autoclave under the conditions of 21MPa, maintenance for 24 hours, then takes out rear service-test machine and measures its elastic recovery capability, evaluation criterion
It is the recovery value of compression distance after discharge degree, compression sample original dimension is 50mm × 50mm × 50mm, initial volume
125cm3.Test result is as shown in table 5.
The elastic property for the preposition gel solidification module that 5 Examples 1 to 8 of table obtains
| Case | Compression distance/mm | Δ V compression volume/cm3 | Compression ratio/% | Rebound degree/% |
| Embodiment 1 | 10 | 25 | 20 | 100 |
| Embodiment 2 | 10 | 25 | 20 | 90 |
| Embodiment 3 | 10 | 25 | 20 | 85 |
| Embodiment 4 | 10 | 25 | 20 | 85 |
| Embodiment 5 | 10 | 25 | 20 | 100 |
| Embodiment 6 | 10 | 25 | 20 | 90 |
| Embodiment 7 | 10 | 25 | 20 | 85 |
| Embodiment 8 | 10 | 25 | 20 | 90 |
As shown in Table 5, the experimental results showed that, different degrees of compression is carried out to gel, gel restores former after removing pressure
Stateful, embodiment 1,5 elastic restoration ratios are 100%.It can thus be appreciated that there is the gel rubber system good elasticity and elasticity to restore
Ability.
Examples 1 to 8 density is 1.9g/cm by simulation wellbore hole3Gel slurry pour the steel cylinder for being filled in Φ 50mm × 100mm
It in mold, is conserved under the conditions of certain temperature and tests cementing strength for 24 hours, test result is as shown in table 6.
6 gel solidification module gel cementation performance of table
As shown in Table 6, after the completion of cementing strength test, it can be seen that nearby gel is destroyed cement plane, still there is gel residue
On viscous glutinous test wall, it is seen that it is excellent with steel wall bonding capacity.
Influence to preposition gel to the rheological property of hydrogel is studied, and test result is respectively such as 8 institute of table 7 and table
Show, the test temperature of table 7 is 80 DEG C, and the test temperature of table 8 is 90 DEG C, wherein φ 600, φ 300, φ 200, φ 100,6 and of φ
φ 3 is different rotating speeds.
Influence of the 7 preposition gel of the present invention of table to the rheological property of cement slurry
Influence of the 8 preposition gel of the present invention of table to the rheological property of cement slurry
According to the ratio and test condition of table 7 and table 8, various ratio slurries as in water-bath for 24 hours after it is curable.Knot
Rheological property data in table 7 and table 8 are closed it is found that preposition gel and cement slurry are according to various ratios at a temperature of 80 DEG C with 90 DEG C
Mixing after, streamline performance influence less, it is Bingham model fluid that reheology model, which has not been changed, and rheological property is good, not shadow
Ring pumping.
As seen from the above embodiment, provided by the invention to cement the well with the intensity of preposition gel, rheological property, stability all
Very well, reliable construction guarantee is provided for prevention annular space is with pressure, from prevention also without larger impact to the thickening time of cement slurry
Annular space angle with pressure, the gel rubber system have broad application prospects in casing and cementing.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preposition gel of well cementation, the component comprising following mass parts：
The preparation method of epoxy resin includes the following steps in the epoxy resin solution：
(1) epoxy propane butyl ether, butyl acrylate, phloroglucin and deionized water are mixed, carries out polycondensation reaction, obtains ring
Oxygen resin precursor；The temperature of the polycondensation reaction is 80~90 DEG C, and the time of polycondensation reaction is 3.5~4.5h；
(2) the epoxy resin precursor that the step (1) obtains is mixed with alkaline solution, carries out ring-closure reaction, is reacted
Feed liquid；The temperature of the reaction is 83~87 DEG C, and the time of reaction is 2.5~3h；
(3) reaction material liquid that the step (2) obtains successively is washed and is dried, obtain epoxy resin.
2. the preposition gel of well cementation according to claim 1, which is characterized in that step (1) the oxypropylene butyl
Ether, butyl acrylate, phloroglucin and water mass ratio be (14.9~15.1)：(14.9~15.1)：(29.9~30.1)：
(19.9~20.1).
3. the preposition gel of well cementation according to claim 1, which is characterized in that the mass concentration of the alkaline solution is
30%；With the meter of the epoxy resin precursor preparation epoxy propane butyl ether, the alkaline solution and propylene oxide fourth
The mass ratio of base ether is (5.9~6.1)：(14.9~15.1).
4. the preposition gel of well cementation according to claim 1, which is characterized in that the resin curing agent is solid for organic amine
Agent.
5. the preposition gel of well cementation according to claim 4, which is characterized in that the organic amine curing agent includes fat
One of race's amine, polyamide and aromatic amine are a variety of.
6. the preposition gel of well cementation according to claim 1, which is characterized in that the retarder include sodium glucoheptonate,
One of boric acid, xylonic acid and acid-co-maleic acid are a variety of.
7. the preposition gel of well cementation according to claim 1, which is characterized in that the swelling agent includes sodium hydroxide, silicon
One of alunite, calcium sulphoaluminate, calcium oxide, fe and calcium oxide-calcium sulphoaluminate compound is a variety of.
8. the preposition gel of well cementation according to claim 1, which is characterized in that the emulsifier is aliphatic alcohol polyethenoxy
Ether compound.
9. the preposition gel of well cementation according to claim 1, which is characterized in that the heavy weight additive includes barite or iron ore
Powder.
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| JP7005072B1 (en) | 2021-04-13 | 2022-01-21 | ▲広▼州大学 | Low-temperature curing type high-strength coated sand material and its manufacturing method |
| CN115504713A (en) * | 2022-09-09 | 2022-12-23 | 长江大学 | Pre-cured resin-based cement slurry with high cementing toughness for shaft plugging as well as preparation method and application thereof |
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Application publication date: 20181116 |